Detection limit. In spectrophotometry, we measure the concentration of an analyte by its absorbance of light. A low-concentration sample was prepared and nine replicate measurements gave absorbances of 0.0047,0.0054,0.0062,0.0060,0.0046,0.0056,0.0052,0.0044, and 0.0058. Nine reagent blanks gave values of 0.0006,0.0012, 0.0022,0.0005,0.0016,0.0008,0.0017,0.0010, and 0.0011.

a) Find the absorbance detection limit with equation 5-3.

b) The calibration curve is a graph of absorbance versus concentration. Absorbance is a dimensionless quantity. The slope of the calibration curve is m=2.24x104M-1Find the concentration detection limit with Equation 5-5.

(c) Find the lower limit of quantitation with Equation 5-6.

Short Answer

Expert verified

a) The absorbance detection limit of the sample was calculated as

0.003112.

b) The minimum detectable concentration of the sample was calculated as

8.6x10-8M.

c) The lower limit of quantitation of the sample was calculated as

2.9x10-7M

Step by step solution

01

Concept used

Detection limit:

This is the concentration of an analyte that produces a signal which is equal to three times the standard deviation of a signal from a blank.

The absorbance detectable concentration ydlcan be defined as,:

signal detection limitydl=yblank+3s

Minimum detectable concentration=3sm

Lower limit of quantitation=10sm

Where,

s=Standard deviation.

m=Slope of linear calibration curve.

02

Calculate the absorbance detection limit of the sample

a)The low concentrations samples near the detection limit are.

0.0006,0.0012,0.0022,0.0005,0.0016,0.0008,0.00017,0.0010,0.0011.

The mean reading of the nine blanks is 0.001189.

The calculated standard deviation of the nine samples is 0.000644.

ydl=yblank+3sydl=0.00118+30.00688=0.022

03

Calculate the minimum detectable concentration of the sample

b)The low concentrations samples near the detection limit are. 0.0006,0.0012,0.0022,0.0005,0.0016,0.0008,0.00017,0.0010,0.0011.

The mean reading of nine blanks is 0.001189.

The slope of the calibration curve is 2.24x104M1

The calculated standard deviation of the nine samples is 0.000644.minimumdetectableconcentration=3sm

=30.0006442.24x104M-1=8.6x10-8M

04

Calculate the lower limit quantitation of the sample

c)The low concentrations samples near the detection limit are.

0.0006,0.0012,0.0022,0.0005,0.0016,0.0008,0.00017,0.0010,0.0011.

The mean reading of nine blanks is 0.001189.

The slope of the calibration curve is 2.24x104M-1.

The calculated standard deviation of the nine samples is 0.000644.

lower limit of quantitation

Lowerlimitofquantitation=10sm=100.0006442.24x104M=2.9x107M

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Most popular questions from this chapter

Europium is a lanthanide element found at parts per billion levels in natural waters. It can be measured from the intensity of orange light emitted when a solution is illuminated with ultraviolet radiation. Certain organic compounds that bindEu(III)are required to enhance the emission. The figure shows standard addition experiments in which10.00mLof sample and20.00mLcontaining a large excess of organic additive were placed in 50-mL volumetric flasks. Then Eu(III) standards (0,5.00,10.00,or15.00mL) were added and the flasks were diluted to50.0mLwithH2O. Standards added to tap water contained0.152ng/mL(ppb) of Eu(III), but those added to pond water were 100 times more concentrated (15.2 ng/mL).


(a) Calculate the concentration of Eu(III)(ng/mL) in pond water and tap water.

(b) For tap water, emission peak area increases by.4.61units when 10.00mL of 0.152ng/mL standard are added. This response is4.61 units/1.52ng = 3.03units per ng ofEu(III). For pond water, the response is12.5units when10.00mLof15.2ng/mLstandard are added, or0.0822units per ng. How would you explain these observations? Why was standard addition necessary for this analysis?

Standard addition graph. Students performed an experiment like that in Figure 5-7 in which each flask contained 25.00mLof serum, varying additions of 2.640MNaCIstandard, and a total volume of 50.00mL.


(a) Prepare a standard addition graph and find [Na+]in the serum.

(b) Find the standard deviation and 95%confidence interval for [Na+].

Internal standard calibration curve. Figure 5-10 is a graph of Ax/Asversus[X]/[S]=(mol%vinylacetateunits)/(mol%ethyleneunits)=q/p in Reaction 5-13.

(d) From the uncertaintyubof the intercept, find the95%confidence interval for the intercept. Does this interval include the theoretical value of zero?

What is the difference between a false positive and a false negative?

In a murder trial in the 1990 s, the defendant's blood was found at the crime scene. The prosecutor argued that blood was left by the defendant during the crime. The defense argued that police "planted" the defendant's blood from a sample collected later. Blood is normally collected in a vial containing the metal-binding compound EDTA (as an anticoagulant) at a concentration of ~4.5mMafter the vial is filled with blood. At the time of the trial, procedures to measure EDTA in blood were not well established. Even though the amount of EDTA found in the crime-scene blood was orders of magnitude below ~4.5mM

, the jury acquitted the defendant. This trial motivated the development of a new method to measure EDTA in blood.

(a) Precision and accuracy. To measure accuracy and precision of the method, blood was fortified with EDTA to known levels.

Accuracy=100×meanvaluefound-knownvalueknownvaluePrecision=100×standarddeviationmean=coeffcientofvariation

For each of the three spike levels in the table, find the precision and accuracy of the quality control samples.

(b) Detection and quantitation limits. Low concentrations of EDTA near the detection limit gave the following dimensionless instrument readings: 175,104,164,193,131,189,155,133,151, and 176. Ten blanks had a mean reading of 45 - 1 . The slope of the calibration curve is1.75×199M-1. Estimate the signal and concentration detection limits and the lower limit of quantitation for EDTA.

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